‘US 2008)
1
48653.
cu») United States
cz) Patent Application Publication — co) Pub. No.: US 2008/0148653 Al
Bauer et al. (43) Pub. Date Jun, 26, 2008
(54) SUBMICRON ALPHLA ALUMINA 1 Related
TEMPERATURE BONDED ABRASIVES
Application Data
(60) Provisional application No, 60(870,740, ile on Dee.
(75) Inventors: Ralph Bauer, Niagara alls (CA): eae
Margaret L. Skowron, Nisgara Publication Classification
Falls, NY ( 5
G1) Inve,
Comespondence Address BUD 300 (2006.01)
LARSON NEWMAN ABEL POLANSKY & — (52) US.Cl 51309
LP. :
TCOURTYARD DRIVE, SUITE 200") ABSTRACT
AUSTIN, TX 78730 A high temperature bonded abrasive inchades alumina aba
sve grits, and a vitreous bond matrix in which the alumina
(73) Assignce: SAINEGOBAIN CERAMICS & —_abrasivegrts are distribted, the vtreousbond matrix having
PLASTICS, INC, Woreest ‘cue temperature not less than 1000” C, The alumina ab
(ws) ive grits include polycrystalline alpha alumina having a fine
erystalline mirosteuctre characterized by an alpha alumina
Appl.No: 11984,735 average domain size not greater than SO0 am, and the alumina
abrasive grits futher include a pinning agent tat is a dis
File Dee. 12,2007 persed phase in the polyerystlline alphs aluminaUS 2008/0148653 Al
SUBMICRON ALPHA ALUMINA HIGH.
‘TEMPERATURE BONDED ABRASIVES
‘CROSS REFERENCE TO RELATED
"APPLICATIONS,
{0001} The present application elsims priority from US.
Provisional Patent Application No. 60/870, 740, fled Dec. 19
2006, entitled "SUBMICRON ALPHA ALUMINA HIGH
TEMPERATURE BONDED ABRASIVES®, naming inven
‘ors Ralph Bauer and Margaret L, Skovsron, which appli
tion is incorporated by reference herein i its entirety.
BACKGROUND
[0002] 1. Field ofthe Disclosure
[0003] Aspects of the present invention are generally
slirected to high temperature bonded abrasive tools and come
ponents, particularly, high temperature Bonded abrasives that
Incomporate fine microstructure alumina abrasive gris.
[0004] 2. Description of the Related Ar
0005) High perfomance abrasive materials and compo-
rents have Tong bees used in various indistal-machining
applications, inctuding lapping/grindng, in which bulk mate-
ial removal is executed, to fe polishing, in which fine
‘micron and submicron surface integularties are addressed.
Typical materials that undergo such machining operations
include various ceramics, lasses, glass-ceramics, metals and
imetalalloys. Abrasives may tke on any one of various fons,
such as fse abrasives as in an abrasive shury in which loose
abrasive particles in suspension are used! for machining.
Altematively abrasives may take the form of fixed abrasive,
such asa coated abrasive or a bonds! abrasive, Coated abe
fives are generally categorized as abrasive components fa
jing an underlying substrate o Which abrasive grits or grains
are adhered therto through a series of make coats and size
‘oats. Bonded abrasives typivally donot have an underlying
Substrate and are formed of integral siniture of abrasive
tits that are bonded together via a matrix bonding materi
10006] Sta of dae ar bonded abrasives ake advantage of
vitreous bonding material, such as siliea-baed glass bond:
ing matrices, Altemativey, specialized honded abrasives for
‘certain applications incorporate superabrasive ais, such as
‘cubic boron carbide and diamond, and may be integrally
bonded through the use of a metal alloy bond max.
10007] While bonded abrasives have continued to undergo
‘development in recent years, particular attention hiss been
pid high temperature bonded abresives that uilize a bond-
{ng matex formed of a vitreous material. An example of &
high temperature honded abrasive component is described ia
US. Pat. No. $282,875. While state of the art high temipera-
ture bonded abrasive components have improved perfor-
mance and durability, a need continues to exist in the at for
Jurther improved components,
SUMMARY,
10008] According to one aspect, high temperature bonded
abrasive is provided that includes alumina abrasive grits and
‘a vitveous Bond matrix in which the abrasive pits are distrib
ted, The vitreous bond matrix has high temperature proper
tis, inclutinga.cure temperature no Tess than about 1000°C.
‘The alumina abrasive grits comprise polycrystalline c-ali-
‘ming having a fine crystalline microstructure characterized
by an ccalumina average domain size not greater than S00
1am. The alumina abrasive prits futher comprise a pinning
Jun. 26, 2008
‘agent, the pinning agent comprising a dispersed phase i
polyerystalline -lumina phise
[0009] According to another aspect, » high temperature
‘bonded abrasive is provided that includes alumina abrasive
arts and vitreous bond matix in which the gris are distib-
‘uted. The vteeous bond maitx has cute temperatre not less
than 1000" C. The alumina abrasive grits comprise polyerys-
‘alline c-alumina having a fine crystalline microstructure
characterized by an average domain size of not greater than
300 nm, Further, the aluaiina abrasive gris eonipise a pin-
fing dgent including at least a zirconium oxide phase di
persed inthe polyerystalline a-alumina phase.
[0010] In addition, a method for forming a high tempera
ture bonded abrasive is provided, The method cals for form-
‘ng fine crystalline microstructure c-aumina abrasive grits
by heat-treating c-alumina precursor containing a pinning
‘agent ata temperature not less than 1350° C. A shaped body
is then formed containing the c-alumina grits and a vitreous
‘bond matrix material. Further, heat treatment of the sbapod
body is earried out ata eure temperature not less than 1000°
Coad above the melting point of the vitreous bond matrix
‘material. The alumina abrasive prits have an average erystal-
line domsin size not greater than about 300 nm after be
tecating,
DESCRIPTION OF THE EMBODIMENTS
[011] According to an embodiment, high-temperature
bonded abrasive inchudes alumina abrasive grits that have a
particularly’ fine mierostucture ala viteous boad mati in
‘which the alumina abrasive grits ar distribute.
[0012] Taming first 0 a description ofthe alumina abrasive
arts, typically the alumina abrasive grits are principally
ormed of polycrystalline cealumina, The polyerystalline
‘calumina generally forms the majority phase ofthe sits,
that sat least 50% by weight. Hawever, generally the al
‘mina abeasve grits are at least 60 wt. %, oftentimes at least 80
‘wt %, and in certain embodiments at least 90 wt. % poly-
enystalline c-alumina. The polyerystalline a-alumins has
Tine erytalline mierosirucure that may be characterized by
an aalumina average domain size not greater than S00 um.
‘The erystaline domains are discrete ideatifiable erytalline
regions of the microstructure that are formed of an agarega-
tion of single erystals, or may be formed ofa single erystal.
However, according to certain embodiments, the erytalline
domains are monocrystalline andar easily observed tough
scanning electron microscopy analysis. The erystalline
domain size may be even fines, such a not greater than 400
‘im, or not greater than 300 nm. With the even finer erystal
domain size, typically the domains are single erystalline as
‘noted above. Stch fine domains may be particularly small,
stich as not greater than 200/nm, aot greater than 190 nem, oF
{even not greater than 180 nm. Its notewony thatthe fine
enystalline domain size is present in the high temperature
‘bonded abrasive component, postprocessing. Thisispariew-
larly noteworthy, as ofientimes the process for Forming the
high temperature bonded abrasive involves high temperature
iwatment at which the vitreous bond matrix cures. Sich high
temperature treatment has a tendency t0 cate domain
growth, which is particularly undesirable. Further detils are
provid elo:
0013] As noted above, the alumina abrasive grits further
include pinning agent. pinning agent isa material that isUS 2008/0148653 Al
‘oreign tothe a-aluminss microstricture ofthe grits, and ea
be identified by a second phase dispersed in the polyenystal-
line a-alumins matrix phase. The pinning agent is generally
‘effective to “pin” the domains, thereby preventing exagger-
‘ated domain growth during sintering andor high temperature
processing of the prits to form the bonded abrasive compo-
nent. Examples of a pinning agent include oxides, carbides
nitrides and borides, as well as reaetion products thereof with
thepolyerystalline alumina matzix. According wo parcular
‘embodiments, the pinning agent comprises an oxide of at
Jeast one of silicon, boroa, tanium, zirconium, and a rare-
‘earth element, and reaction products thereof with the poly
‘eqstalline cealumina matrix. A particular pinning agent is
‘rconium oxide, generally in the form of ZrO, (zirconia).
Zirconium oxide is particularly suitable material, and gener-
allyis inert within te polycrystalline -alumina mate, s0as
to undergo very limited reation with the alumina thereby
retaining a zirconium oxide crystal phase, typically zirconia
‘Thepinning agent is generally prescat in the alumina abrasive
‘fis in an amount not less than about 0.1 w. %, such as an
amount not less than about 0.5 wt. %, oF not less than about
1.Owt, %, The lower limit ofthe pinning agent is chosen to be
an amount that is effective to prevent exaggerated! domain
row
{0014} According to one embodiment, the pinning agent is
present in the abrasive grit in an amount not preser than 40
14%, suel. as am amount not greater than 30 wt. %, not
nvater than 20 wt. % or even not greater than 10 wt. %. Inthe
high temperature bonded abrasive, the pinning agent is gen-
‘erally identified as having a particulate size not greater than S
microns, seh as aot greater than | micron, Fine particulate
sizes associated with the pinning agent have been found to be
useful such as aot greater than S00 am, or not greater than
300 nm, or not greater than 200 nm. As deseribed in more
detail below, in the context of methods for forming high
temperature bonded abrasive components, the pinning agent
‘may be intzoduced into the alumina abrasive gris ia solid
orm, such as in sub-micron form, particularly including col-
Joidal form. Alternatively, the pinning agent may be intro-
‘duced into the alumina abrasive grits oF precursor thereo
such that upon high temperature heat twatment the pinning
‘agen precursor converts into a desired crystalline phase sch
asthe desired oxide, carbide, nitride or boride
[0015] Processing o form high temperature bonded abea-
sive according to embodiments ofthe present invention gen-
‘erally begins withthe Formation ofthe alumi abrasive ris
‘According to particular embodiment, the alumina abrasive
_ritsare formed through ascodedl proces, in which an appro=
priate seding material is combines with an c-alumina pre-
‘cursor, followed by heat treatment fo convert the alumina
precursor into the desired c-alumina phase. The seedsmay be
Tormed in accordance with U.S, Pat No. 4,623,364, in which
coded gel alumina dried precursor is calcined o form c-ali-
ming. The calcined c-alumina may be further processed such
asby milling to provide an appropriate high-surface area seed
material. Typically the surface are is quantified by specific
surface area (SSA), not less than 10 mig typically not less
than 20m/g, suchas not less than 30s", oF not Tess than 40
Panicular embodiments have a surface area not less
than 50 m/g, Generally, the surface area is limited, such as
not greater than 300 mp, such as not greater than 250 mfg.
Jun. 26, 2008
{0016} The seed materials then combined with the she
‘mina procure, which may take on anyone of several ors
of alminous terials tht is an appropriate form for con-
version 1 cealumina, Such prccurce materials inlode for
example, hydrated aluminss, including alumina wiydeate
(ATH) and boohmite. As usd herein, bochnite denotes aie
sina Iydrates inching sineral bochaite, typically being
AI,Oy H,0 and having a water content onthe order of 15%
as well as pseudo-bochmite, having water content greater
than 18%, suc as 209610 38%. As auch the tem boehiit
willbe used t denote alumina hydrates having 15 10 38%
wate comtent, suchas 15 to 30% water content by weight It
js noted that bochmite, inching pseudo-boehmite, has a
paticularand identifiable erystalstictre and accontingly a
‘nique X-ray action patter, and as sch, is distinguished
from olher aluminous materials, including ether hydrated
alominas
{0017} ‘Typically, the a-aumina precursor, such as boeh-
ites combined with th sod ansterialsuch that the seeds
fre presen in an mount aot es than 0.2 wt with respect
{0 tal solids content of seeds and qcaluminn precursor
Typically, the seas are present in aout less han 30 wt
°%.or. typically, nan aroun not greater than 20 wt 9%
{0018} "Theseedsndthe calunina peecurorare generally
combined in sly form which thea gle, such bythe
fddtion of an appropriate acd or hase seh a aie acid
Following gelation, the gels typically dried, crashed, and
hicd material is posse though classification sieves. The
elastied soid ation may then be subjected to sintering
process that has imited soak time. Typically, sintering is
famed our fra time period not exceeding, 30 minutes, such
‘snot greater than 20 minutes, not gretee than 15 mines
According to particular embodiments the sintering period i
particularly shor, suc as not rete than 10 minutes
{0019} According o a particuar development, pining
‘gent oe pining agent pescsoe is ade tothe sispension
containing seeds and alumina recurso. Type the pin-
geal rFting age recs is present in. au
ot greater than 40 wt % based upon the combined solids
content of he c-alumisa pressor, seeds, ad pining agent
rim agent prursorcalulted bas upon sols con-
tent ofthe pinning agent in he final ealumina rit). Gener
ally thepiingagents preset ina amount ot shan
‘wt 9%, such as not Tess than about 05 wt % or even not ss
than about 1 wt. %, based upon the total Solids content as
noted above
{0020} Sil func, seconding to a particular development
Sintering searied outta temperature above the emperatire
that is necessary to effect conversion of the alumina pre
cursor into cealumina, Ina sense, certain embodiments eal
for “oveesntring” the alumina procrsor mister. Pat
ticularly suitable temperatures are generally not less than
1380° C, sch ak not es than 1378" C., not less than 1385°
mot less than 198°C. or aot less than 1400” C. In this
respect, it noted that while ne microsritured seeded
Ccalimina materials have boca formed in the atypically
such materials are processed at lower temperatures, ofen-
times below 1380" C:, such as on the onder of 1300" C
Further observations on the combined eect of utilization of
a pining agen andoversnteringare provided herein below.US 2008/0148653 Al
10021] Following sintering, optionally classified abrasive
_ritsare then combined witha vitreous bond material, shaped
Jno.an appropriate geometric eontour (eg. grinding whe),
which contoursand shapes ae well appreciated inthe context
‘of the bonded abrasives at. Processing 10 complete the
bonded abrasive component typically involves heat treatment
at a cure temperature. As used herein, cure temperature
‘denotes a material parameter associated with the vitreous
bond matrix material andi generally in excess ofthe melting
temperature, and particularly, the glass transition temperature
“Tofthe bonding material The eure temperature isthe mii
lun temperature at which the bond matrix material not oaly
softens and becomes flowable, but also becomes flowable 10
fn extent ensuring complete wetting and honing to the abra-
sive gris. Typically, the cure temperature aevording 10
ubodliments herein isnot ess haa 1000° C, generally indi
‘cating formation ofa high temperature bonded abrasive
10022] Particular examples were made according to the
following description.
EXAMPLES
Example 1
Comparative
10023] In 400 mil pyrex beaker, 30 grams of aluminum
‘oxide hydroxide (pseudo boehiite) powder under the trade
name DISPERAL obtained from Sasol Ine of Hamburg Ger
‘many was sired into 61 milliliters of deionized water (ress-
tivity 2 mega-ohm em),
10024] Asa seed feedstock, seeded gel alumina dried pre-
‘cursor as propre in US, Pa. No, 4,623,364 was calcined at
1100 for$ minutes ina rotary kiln to convert the alumina to
form with asurfacearea as measured by the BET method of
15 to 28 m’/g. 72 kg ofthis cvaluinina feedstock was mixed
“with 150kgof deionized water and fed ito horizontal bead,
mill manufactured by Netz Company (headquarters Selb
‘Germany The model ofthe device was LMZ-25. Milling
was conducted for 24 hours with the slurry continuously